CN105441983B - A kind of preparation method of crome metal - Google Patents
A kind of preparation method of crome metal Download PDFInfo
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- CN105441983B CN105441983B CN201510799602.2A CN201510799602A CN105441983B CN 105441983 B CN105441983 B CN 105441983B CN 201510799602 A CN201510799602 A CN 201510799602A CN 105441983 B CN105441983 B CN 105441983B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/32—Electrolytic production, recovery or refining of metals by electrolysis of melts of chromium
Abstract
The present invention provides a kind of preparation method of crome metal, the preparation method is：Under an inert atmosphere, the substance formed using calcium chromium oxygen prepares crome metal as cathode using FFC Cambridge process electrolyte.The substance of the calcium chromium oxygen composition is preferably chromous acid calcium (CaCr2O4) pure material, the substance of the calcium chromium oxygen composition is by calcining to obtain the mixture of chrome green and calcium oxide.Current efficiency is high during the method prepares crome metal, up to 60%；It is fast to be electrolysed rate, it is only necessary to which 2h can obtain crome metal；And the crome metal purity being prepared is high, and the purity of crome metal reaches 99.2%, oxygen content 0.1%.
Description
Technical field
The invention belongs to technical field of electrochemical metallurgy, be related to a kind of method for preparing crome metal more particularly to it is a kind of with
The method that the substance of calcium chromium oxygen composition prepares crome metal for cathode using FFC Cambridge technique.
Background technology
Crome metal product is mainly obtained using aluminothermic reduction at present, consumes a large amount of precious metal aluminium powders, and mistake in the process
Lead to the introducing of aluminium, iron tramp in journey, the crome metal product purity of preparation is relatively low.In addition aqueous solution electrolysis prepares crome metal product
Evolving hydrogen reaction is often accompanied by, causes current efficiency low, electrolytic production has Hydrogen Brittleness Phenomena.
In recent years, the FFC process electrolytes developed with Cambridge University prepare the further investigation that metal causes many scholars, this electrolysis
Method can prepare numerous metals such as titanium, chromium, tantalum, niobium and alloy, if George et al. is with Cr2O3For cathode, using graphite as anode,
With CaCl2Fused salt is electrolyte, and 4h is electrolysed under the voltage of 2.7-2.8V, and crome metal (Direct has been prepared
Electrolytic preparation of chromium powder, Metallurgical and Materials
Transactions B, 2004,35 (2)：223-233)；CN 104372380A disclose a kind of low-temperature molten salt method prepare it is high-purity
The method of chromium, the method includes following steps：First, prepare high-purity chromium trichloride solution, isolate major impurity from
Son；Then, anhydrous chromium trichloride crystal is prepared；Next, prepare low-temperature molten salt system；Finally, by trichlorine in low-temperature molten salt
Change chromium electrolytic preparation High Pure Chromium；CN 102505128A disclose a kind of method that molten-salt electrolysis directly prepares porous metal article,
This method is：Using metal stock as cathode, graphite is anode, CaCl2For electrolyte, the molten-salt electrolysis under argon gas protective condition
4h-30h obtains the porous metal article that porosity is 15%~78%；The temperature of the electrolysis is 850 DEG C -1200 DEG C, electrolysis
Voltage be 2.8V-3.8V；The metal stock is using metal oxide powder as raw material, and pore creating material is added using conventional method
The metal stock prepared by compacting and sintering.
But during preparing crome metal using electrolysis, often find exist with the metal salt intermediate product of calcium, from
And causing electrolysis rate slack-off, current efficiency reduces.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of preparation method of crome metal, utilize
The method, which prepares crome metal, has many advantages, such as that current efficiency is high, electrolysis rate is fast and crome metal purity obtained is high.
For this purpose, the present invention uses following technical scheme：
A kind of preparation method of crome metal, the preparation method are：Under an inert atmosphere, using the substance that calcium chromium oxygen forms as
Cathode prepares crome metal using FFC Cambridge process electrolyte.
The substance of the calcium chromium oxygen composition refers to the substance that component is calcium, chromium and oxygen, the object of the calcium chromium oxygen composition
Matter can be pure substance or mixture.
The substance of the calcium chromium oxygen composition is CaCr2O4And/or Ca2Cr2O5Or, Cr2O3With CaCr2O4And/or Ca2Cr2O5
Mixture.The substance of the calcium chromium oxygen composition can be CaCr2O4, Ca2Cr2O5, CaCr2O4With Ca2Cr2O5Mixture, Cr2O3
With CaCr2O4Mixture, Cr2O3With Ca2Cr2O5Mixture, Cr2O3、CaCr2O4With Ca2Cr2O5Mixture in it is any one
Kind, preferably pure chromous acid calcium (CaCr2O4)。
The substance of the calcium chromium oxygen composition is by calcining Cr2O3It is obtained with the mixture of CaO.
Preferably, the Cr2O3Molar ratio with CaO is 1:0.1-1:1, such as 1:0.2、1:0.3、1:0.4、1:0.5、1:
0.6、1:0.7、1:0.8 or 1:0.9 etc..
Preferably, the temperature of the calcining be 1000-1400 DEG C, such as 1050 DEG C, 1100 DEG C, 1150 DEG C, 1200 DEG C, 1250
DEG C, 1300 DEG C or 1350 DEG C etc., preferably 1100-1300 DEG C；
Preferably, the time of the calcining is more than 1h, such as 1.5h, 2h, 2.2h, 3h, 3.5h, 4h, 5h, 6h or 10h, excellent
It is selected as 2-3h.
Preferably, the calcining carries out under air or inert atmosphere.
Preferably, the substance of calcium chromium oxygen composition is by under an inert atmosphere, by calcium oxide and chrome green in chlorine
Change and be obtained by the reaction in calcium fused salt.The preparation method is preferably：Under an inert atmosphere, it is 2 by molar ratio:1-3:1 calcium oxide
1-4h is reacted in calcium chloride fused salt with chrome green, the temperature of reaction is 850-950 DEG C, and later, reaction product is washed,
It is dry.
The inert atmosphere can be nitrogen atmosphere or inert gas atmosphere.The inert atmosphere is preferably argon gas atmosphere, nitrogen
One kind or at least two combination in gas atmosphere or helium atmosphere.Typical but non-limiting inert atmosphere is combined as：Argon gas
With nitrogen atmosphere, nitrogen and helium atmosphere, argon gas and helium atmosphere, argon gas, nitrogen and helium atmosphere.
The substance of the calcium chromium oxygen composition is porous blocks.The size of the porous blocks according to amount of electrolyte not
Together, and its diameter is changeable.The substance that the calcium chromium oxygen of porous blocks is formed is carried out directly as cathode under the function of current
Electro-deoxidation reduction process, calcium ion are dissolved into fused salt, and final cathode block leaves crome metal product, and this addresses the problem calcium chromium
The problem of material demand of oxygen composition dissolves in fused salt, while the yield basic 100% of elemental chromium.
Preferably, the porous blocks are prepared by the substance tabletting that forms calcium chromium oxygen, sintering.
Preferably, the pressure of the tabletting be 100-170MPa, as 105MPa, 110MPa, 120MPa, 130MPa,
140MPa, 150MPa, 160MPa or 165MPa etc.；
Preferably, the temperature of the sintering be 800-1400 DEG C, such as 850 DEG C, 900 DEG C, 950 DEG C, 1000 DEG C, 1100 DEG C,
1150 DEG C, 1200 DEG C, 1250 DEG C, 1300 DEG C or 1350 DEG C etc., preferably 1000-1200 DEG C.
Preferably, the time of the sintering is more than 1h, such as 1.5h, 2h, 3h, 4h, 5h, 6h, 10h or 20h, preferably 2-
3h。
The electrolyte used that is electrolysed need to be the preferable fused salt of dissolved oxygen ability, preferably calcium chloride fused salt or calcium chloride
Base fused salt, more preferably calcium chloride fused salt.
Preferably, the calcium chloride base fused salt by calcium chloride fused salt and alkali metal chloride and/or alkaline-earth metal
Chloride forms.The mass ratio of the chloride of the chloride and/or alkaline-earth metal of calcium chloride fused salt and alkali metal is arbitrary ratio.
During electrolysis, the substance of the calcium chromium oxygen composition, quality 1.5g.
Preferably, the voltage of the electrolysis is 2.5-3.5V, such as 2.5V, 2.7V, 2.9V, 3.0V, 3.1V, 3.3V or 3.4V
Deng preferably 2.8-3.2V.
Preferably, the time of the electrolysis is 2-8h, such as 2h, 4h, 6h or 7h.The electrolysis time and cathode quality and
Decomposition voltage is related, selects different cathode quality and decomposition voltage, required electrolysis time is different, and those skilled in the art can
It is voluntarily adjusted in practical operation.
The temperature of the electrolysis is higher than the fusing point of electrolyte.
Preferably, the temperature of the electrolysis is 100-200 DEG C higher than the fusing point of electrolyte, such as higher than electrolyte fusing point 110,
120th, 130,140,150,160,170,180 or 190 DEG C etc..
The anode of the electrolysis is graphite electrode, and the corrosion resistance of graphite electrode under the high temperature conditions is excellent, will not be by
Corrosion, will not pollute the crome metal being prepared.
The cathode further includes conductive current collector, and the conductive current collector is connected with the substance that calcium chromium oxygen forms.The calcium
The substance of chromium oxygen composition and the connection mode of conductive current collector are：It perforates on the substance of calcium chromium oxygen composition, by conductive current collector
Across hole.
The conductive current collector conducts electricity very well, and fusing point is more than the fusing point of molten salt electrolyte, and corrosion-resistant, the conduction
Collector is preferably stainless steel wire, molybdenum filament, tungsten filament or nickel wire.
As preferred technical solution, the preparation method of the crome metal is：Under an inert atmosphere, it is formed with calcium chromium oxygen
Substance and the compound of conductive current collector are cathode, using graphite as anode, using fused salt as electrolyte, higher than fused salt fusing point 100-
It at a temperature of 200 DEG C, is electrolysed under the voltage of 2.5-3.5V, later, cooling and washs cathode, dry to get to metal
Chromium.
The cooling, washing and dry actual conditions are without specifically limited, as long as the washing can be by metal chromium surface
Fused salt processing it is clean, those skilled in the art can be selected according to the actual state for preparing crome metal cooling temperature and
Time, the solvent of washing and number and the temperature and time of drying.
Compared with prior art, beneficial effects of the present invention are：
(1) current efficiency is high during the preparation method of crome metal provided by the invention prepares crome metal, up to 60%.
(2) the preparation method electrolysis rate of crome metal provided by the invention is fast, it is only necessary to which 2h can obtain crome metal.
(3) the crome metal purity that the preparation method of crome metal provided by the invention is prepared is high, and the purity of crome metal reaches
To 99.2%, oxygen content 0.1%.
Description of the drawings
Fig. 1 is the X ray diffracting spectrum of crome metal obtained that embodiment 1 provides.
Fig. 2 is the stereoscan photograph of crome metal obtained that embodiment 1 provides.
Specific embodiment
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in understanding the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1
Chromous acid calcium powder is made to the sheet body of diameter 13mm, quality about 1.5g in 170MPa lower sheetings, through 1000 DEG C, sky
After being sintered 2 hours in gas atmosphere, it and conductive current collector are combined cathode for electrolyzing；Using graphite as anode, in argon gas gas
Under atmosphere, temperature is in 900 DEG C of calcium chloride fused salt, is electrolysed 2 hours under 3.2V voltages；After electrolysis, solid-state is taken out in cooling
Cathode is washed, dry, you can to obtain crome metal.
Detection and analysis result is shown：Titration determination crome metal purity is about 99.2%, pulsed infrared thermal conductivity oxygen-nitrogen analyzer
It is 0.1% to measure oxygen content, and current efficiency is up to 60%.
It is the X ray diffracting spectrum of product obtained as shown in Figure 1, it can be seen from the figure that diffraction maximum and gold in figure
Belong to the completely the same of chromium, product made from explanation is crome metal.
The SEM pictures of crome metal obtained are illustrated in figure 2, it can be seen from the figure that crome metal obtained predominantly saves
Branch shape, size is in the micron-scale.
Embodiment 2
By chrome green and calcium oxide according to molar ratio 1：1 after mixing, and 3 are sintered in 1000 DEG C, air atmosphere
Hour obtains calcium chromium oxygen mixture；Diameter 13mm, quality about 1.5g is made in 100MPa lower sheetings in gained calcium chromium oxygen mixture
Sheet body, through being sintered 2 hours in 1200 DEG C, air atmosphere, it and conductive current collector are combined cathode for electrolyzing；With graphite
For anode, in a nitrogen atmosphere, temperature is 800 DEG C, molar ratio 1：In 1 calcium chloride-sodium chloride fused salt mixt, 2.8V voltages
Lower electrolysis 4 hours；After electrolysis, solid state cathode is taken out in cooling, washes, dry, you can to obtain crome metal.
Detection and analysis result is shown：Crome metal purity is about 99.1%, and oxygen content is about 0.16%, and current efficiency is reachable
47%.
Using the pattern of crome metal made from scanning electron microscope analysis, as a result show：Crome metal obtained is mainly
Branch shape is saved, size is in the micron-scale.
Embodiment 3
By chrome green and calcium oxide according to molar ratio 1：0.1 after mixing, is sintered in 1400 DEG C, air atmosphere
Obtain within 2 hours calcium chromium oxygen mixture；Diameter 13mm, quality about 1.5g is made in 100MPa lower sheetings in gained calcium chromium oxygen mixture
Sheet body, through being sintered 1 hour in 1400 DEG C, nitrogen atmosphere, it and conductive current collector are combined cathode for electrolyzing；With graphite
For anode, under helium atmosphere, temperature is in 800 DEG C of lithium chloride fused salt, is electrolysed 4 hours under 3.5V voltages；After electrolysis,
Solid state cathode is taken out in cooling, washes, dry, you can to obtain crome metal.
Detection and analysis result is shown：Crome metal purity is about 98.2%, and oxygen content is about 0.9%, and current efficiency is reachable
48%.
Using the pattern of crome metal made from scanning electron microscope analysis, as a result show：Crome metal obtained is section branch
Shape, size is in the micron-scale.
Embodiment 4
Chromous acid calcium powder is made to the sheet body of diameter 10mm, quality about 1.5g in 100MPa lower sheetings, through 800 DEG C, nitrogen
After being sintered 3 hours in gas atmosphere, it and conductive current collector are combined cathode for electrolyzing；Using graphite as anode, in nitrogen gas
Under atmosphere, temperature is 750 DEG C, molar ratio 1：In 1 calcium chloride-potassium chloride fused salt mixt, it is electrolysed 4 hours under 2.5V voltages；Electricity
After solution, solid state cathode is taken out in cooling, washes, dry, you can to obtain crome metal.
Detection and analysis result is shown：Crome metal purity is about 98.4%, and oxygen content is about 0.5%, and current efficiency is reachable
45%.
Using the pattern of crome metal made from scanning electron microscope analysis, as a result show：Crome metal obtained is section branch
Shape, size is in the micron-scale.
Embodiment 5
By chrome green and calcium oxide according to molar ratio 1：0.5 after mixing, is sintered in 1100 DEG C, nitrogen atmosphere
Obtain within 3 hours calcium chromium oxygen mixture；Diameter 13mm, quality about 1.5g is made in 150MPa lower sheetings in gained calcium chromium oxygen mixture
Sheet body, through being sintered 2 hours in 1200 DEG C, nitrogen atmosphere, it and conductive current collector are combined cathode for electrolyzing；With graphite
For anode, under an argon atmosphere, temperature is in 900 DEG C of calcium chloride fused salt, is electrolysed 4 hours under 3.0V voltages；After electrolysis,
Solid state cathode is taken out in cooling, washes, dry, you can to obtain crome metal.
Detection and analysis result is shown：Crome metal purity is about 97.8%, and oxygen content is about 1.1%, and current efficiency is reachable
43%.
Using the pattern of crome metal made from scanning electron microscope analysis, as a result show：Crome metal obtained is section branch
Shape, size is in the micron-scale.
Embodiment 6
By chrome green and calcium oxide according to molar ratio 1：0.8 after mixing, is sintered in 1300 DEG C, nitrogen atmosphere
Obtain within 2.5 hours calcium chromium oxygen mixture；Diameter 13mm, quality is made about in 150MPa lower sheetings in gained calcium chromium oxygen mixture
It and conductive current collector through being sintered 3 hours in 800 DEG C, nitrogen atmosphere, are combined cathode for electrolyzing by the sheet body of 1.5g；With
Graphite is anode, and in a nitrogen atmosphere, temperature is in 900 DEG C of calcium chloride fused salt, is electrolysed 8 hours under 2.5V voltages；Electrolysis knot
Solid state cathode is taken out in Shu Hou, cooling, washes, dry, you can to obtain crome metal.
Detection and analysis result is shown：Crome metal purity is about 96%, and oxygen content is about 1.4%, and current efficiency is up to 40%.
Using the pattern of crome metal made from scanning electron microscope analysis, as a result show：Crome metal obtained is section branch
Shape, size is in the micron-scale.
Embodiment 7
By chrome green and calcium oxide according to molar ratio 1：0.3 after mixing, is sintered in 1200 DEG C, nitrogen atmosphere
Obtain within 1 hour calcium chromium oxygen mixture；Diameter 13mm, quality about 1.5g is made in 150MPa lower sheetings in gained calcium chromium oxygen mixture
Sheet body, through being sintered 2.5 hours in 1100 DEG C, nitrogen atmosphere, it and conductive current collector are combined cathode for electrolyzing；With stone
Ink is anode, and under helium atmosphere, temperature is in 900 DEG C of calcium chloride fused salt, is electrolysed 4 hours under 3.0V voltages；Electrolysis terminates
Afterwards, it cools down, takes out solid state cathode, wash, it is dry, you can to obtain crome metal.
Detection and analysis result is shown：Crome metal purity is about 98.8%, and oxygen content is about 0.4%, and current efficiency is reachable
53%.
Using the pattern of crome metal made from scanning electron microscope analysis, as a result show：Crome metal obtained is section branch
Shape, size is in the micron-scale.
Applicant states, the foregoing is merely the specific embodiment of the present invention, but protection scope of the present invention not office
It is limited to this, person of ordinary skill in the field is it will be clearly understood that any belong to those skilled in the art and taken off in the present invention
In the technical scope of dew, the change or replacement that can readily occur in are all fallen within protection scope of the present invention and the open scope.
Claims (25)
1. a kind of preparation method of crome metal, which is characterized in that the preparation method is：Under an inert atmosphere, with calcium chromium oxygen group
Into substance for cathode, crome metal is prepared using FFC Cambridge process electrolyte；
The substance of the calcium chromium oxygen composition is CaCr2O4And/or Ca2Cr2O5, Cr2O3With CaCr2O4, Cr2O3With Ca2Cr2O5, Cr2O3
With CaCr2O4And Ca2Cr2O5In any one, the substance of calcium chromium oxygen composition is by calcining chrome green and calcium oxide
Mixture obtain, the molar ratio of the chrome green and calcium oxide is 1:0.1-1:1, the calcining is in air or indifferent gas
It is carried out under atmosphere, the temperature of the calcining is 1000-1400 DEG C, and the time of the calcining is more than 1h.
2. preparation method according to claim 1, which is characterized in that the substance of the calcium chromium oxygen composition is pure CaCr2O4。
3. preparation method according to claim 1, which is characterized in that the temperature of the calcining is 1100-1300 DEG C.
4. preparation method according to claim 1, which is characterized in that the time of the calcining is 2-3h.
5. preparation method according to claim 1, which is characterized in that the substance of the calcium chromium oxygen composition passes through in indifferent gas
Under atmosphere, calcium oxide and chrome green are obtained by the reaction in calcium chloride fused salt.
6. preparation method according to claim 1, which is characterized in that the inert atmosphere is argon gas atmosphere, nitrogen atmosphere
Or one kind in helium atmosphere or at least two combination.
7. preparation method according to claim 1, which is characterized in that the substance of the calcium chromium oxygen composition is porous blocks.
8. preparation method according to claim 7, which is characterized in that the porous blocks pass through the object that forms calcium chromium oxygen
Matter tabletting, sintering are prepared.
9. preparation method according to claim 8, which is characterized in that the pressure of the tabletting is 100-170Mpa.
10. preparation method according to claim 8, which is characterized in that the temperature of the sintering is 800-1400 DEG C.
11. preparation method according to claim 10, which is characterized in that the temperature of the sintering is 1000-1200 DEG C.
12. preparation method according to claim 8, which is characterized in that the time of the sintering is more than 1h.
13. preparation method according to claim 12, which is characterized in that the time of the sintering is 2-3h.
14. preparation method according to claim 1, which is characterized in that the electrolyte of the electrolysis for calcium chloride fused salt or
Calcium chloride base fused salt.
15. preparation method according to claim 14, which is characterized in that the calcium chloride base fused salt by calcium chloride fused salt with
And the chloride of alkali metal and/or the chloride of alkaline-earth metal form.
16. preparation method according to claim 1, which is characterized in that the substance of the calcium chromium oxygen composition, matter during electrolysis
It measures as 1.5g.
17. preparation method according to claim 1, which is characterized in that the voltage of the electrolysis is 2.5-3.5V.
18. preparation method according to claim 17, which is characterized in that the voltage of the electrolysis is 2.8-3.2V.
19. preparation method according to claim 1, which is characterized in that the time of the electrolysis is 2-8h.
20. preparation method according to claim 1, which is characterized in that the temperature of the electrolysis is higher than the fusing point of electrolyte.
21. preparation method according to claim 1, which is characterized in that the temperature of the electrolysis is higher than the fusing point of electrolyte
100-200℃。
22. preparation method according to claim 1, which is characterized in that the anode of the electrolysis is graphite electrode.
23. preparation method according to claim 1, which is characterized in that the cathode further includes conductive current collector, described to lead
Electrojet body is connected with the substance that the calcium chromium oxygen forms.
24. preparation method according to claim 23, which is characterized in that the conductive current collector for stainless steel wire, molybdenum filament,
Tungsten filament or nickel wire.
25. preparation method according to claim 1, which is characterized in that the preparation method is：Under an inert atmosphere, with
The substance of calcium chromium oxygen composition and the compound of conductive current collector is cathodes, using graphite as anode, using fused salt as electrolyte, higher than
At a temperature of 100-200 DEG C of fused salt fusing point, it is electrolysed under the voltage of 2.5-3.5V, later, cooling, and cathode is washed, it is dry,
Obtain crome metal.
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| CN106048705B (en) * | 2016-07-19 | 2018-01-16 | 中国科学院青海盐湖研究所 | Foam chromium and preparation method thereof |
| CN106978612A (en) * | 2017-03-16 | 2017-07-25 | 广东省稀有金属研究所 | A kind of metallurgical method of metallic compound |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372380A (en) * | 2014-11-18 | 2015-02-25 | 辽宁石化职业技术学院 | Low-temperature fused salt method for preparing high-purity chromium |
| CN104919089A (en) * | 2012-12-24 | 2015-09-16 | 金属电解有限公司 | Method and apparatus for producing metal by electrolytic reduction |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104919089A (en) * | 2012-12-24 | 2015-09-16 | 金属电解有限公司 | Method and apparatus for producing metal by electrolytic reduction |
| CN104372380A (en) * | 2014-11-18 | 2015-02-25 | 辽宁石化职业技术学院 | Low-temperature fused salt method for preparing high-purity chromium |
Non-Patent Citations (2)
| Title |
|---|
| "Direct Electrolytic Preparation of Chromium Powder";GEORGE Z.Chen等，;《Metallurgical and materials transactions B》;20040430;第35卷(第2期);第223页右栏倒数第1段，第224页右栏第1-2段、倒数第1段，第225页左栏第1-2段，第226页左栏第2段、右栏第2段，图2-3、5 * |
| "掺杂的TiO2阴极对熔盐电解的影响";杜继红 等，;《稀有金属》;20070615;第31卷(第3期);摘要、第337页第1节，第338-339页第2.3-2.4节，图5-6 * |
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